反应详情

Ethylenediamine (1.5 mL, 24 mmol) was added dropwise to a solution of 3-chloro-5-nitrobenzo[d]isothiazole (250 mg, 1.2 mmol) in acetonitrile (1 mL). The reaction mixture was microwaved at 120° C. for 10 min. The reaction mixture was concentrated under reduced pressure. The resulting residue was diluted with water and the aqueous mixture was extracted with ethyl acetate. The organic extract was concentrated under reduced pressure and the crude product was purified by column chromatography, on silica gel, eluting with a mixture of 2% methanol in dichloromethane and selected fractions were combined and concentrated under reduced pressure to yield N1-(5-nitrobenzo[d]isothiazol-3-yl)ethane-1,2-diamine (100 mg) as a yellow solid.

1. customThe reaction mixture was microwaved at 120° C. for 10 min
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. additionThe resulting residue was diluted with water
4. extractionthe aqueous mixture was extracted with ethyl acetate
5. extractionThe organic extract
6. concentrationwas concentrated under reduced pressure
7. customthe crude product was purified by column chromatography, on silica gel
8. washeluting with a mixture of 2% methanol in dichloromethane
9. concentrationconcentrated under reduced pressure